Process for the recovery of the paraffin ingredients from cannel-coals and other similarly-constituted bituminous materials without change in their chemical composition.



ITHOUT CHANGE Patented; Dec. 6,1911%.

A TZORNE Y.

H. WURTZ.

THE PARAFFIN INGREDIENTS FROM GANNEL GOALS AND KROOESS FDR TEE RECOVERY OF OTHER SIMILARLY GONSTITUTED BITUMINOUS MATERIALS W IN THEIR CHEMICAL GOMPOSITION.

APPLIUATIOEI FILED N0v.z1, 1904.

UNITED STATES Pazrnnrr OFFICE.

HENRY WURTZ, or NEWARK, NEW JERSEY, Assrsnoh 'ro AMERICAN onnmonn EDUCTION COMPAN Y, A CORPORATION.

PROCESS FOR THE RECOVERY OF THE PARAFFIN INGREDIENTS FROM CANNEL-COJILS AND OTHER SIMILARLY-CONSTITUTED BITUMINOUS MATERIALS WITHOUT CHANGE IN THEIR CHEMICAL COMPOSITION.

Application filed November following being a fnll,clear, an exact specifieati'on of the process, reference being made to jthe accompanying drawing, showing a r 'tical cross-section of the apparatus, taken {through the center thereof, and to the Let ters Patent of the United States No. 821,323,

granted on my application filed April 13, 1905, Serial No. 255,35 to my assignees, the American Chemical Eduction 'Co., a corporation, on the 22d day of May, 1906, and by means of which or other suitably-com structed apparatus this process'may be carried on, therereinattcr explained.

Canncl coal and similarly constituted materials, contain a very large percentage of hydrocarbons, ranging in consistence from solid parallins to light oils of the same series. These hydrman'bons are intimately mixed with the solid ingredients, carbon and.

imon'ibustiblo mineral substances, which form the basic structure of these materials;

and while they can be. separated from the solid constituents by distillation, they cannot. be recovered by any distilling process, heretofore known, in a chemicallyunchangcd condition, because they are rapidly disso ciated by such temperatures as must, necessarily, be employed in any distillingi process, to expand them sufliciently so t ey may escape from the retort, and'because when in such heated state, these hydrocarbons are extremely susceptible of oxidation, and their Specification o;. Lette1s Patent.

Patented Dec. 6, 1910.

21, 1904. Serial No. 233,706.,

paraffin series, without change or-material l modification in their chemical composition.

Cannel coal and similar bituminous compounds may be compared in respect to the gredients with that of, a fibrous porous comustlblestructure, filled with fat and waxy substances, melted and mixed with roportionate quantities of a more liquid oily substance of corresponding chemicalnature and with some absorbent, mcombustible mineral matter in more or-less pulverized state, and thencooled and compressed; the more fluid, oily, ingredients being in the first instance, and more-largely, absorbed by the pulverized absorbent mineral matter and thus held ter, and both intimately intermingled (absorbed) by the absorbent fibrous structure of ,the fibrous combustible structure. Bitumiquent cooling and simultaneous compression rendered solid and apparently homogeneous. In this process of forming such compounds, no chemical change takes place, and there, fore, by reversing the process of formation, their constituent ingredients may be separated from each other. This is effected by the process of consuming the coal in a furnace. If. such coal is heated sufiieiently in a furnace, to melt the waxy hydrocarbon, the latter separates from the fibrous nonmcltable structure of the carbon, and this carbon combines with the heated oxygen of fluid hydrocarbons are decomposed by the heat, some of their elements consumed, and others are converted into gases. If such coal is thus heated in a hermetically closed retort, the carbon and the oxidable constituents of the hydrocarbons are not so. eonsumed, but if the separation of the hydrocarbons from the carbon of the coal ist-o be effected by such a treatment, the hydrocarbons of the bituminous compound must necessarily be expanded-to such an extent that they decompose, and are largely, if not totally, converted into fixed. gases and other less valuable products. This is't-he unavoidable result of every process of distilling temperatures .(from red heat down to about suspended in the less fluid 'fat or wax matcoals, and while in distilling coal at low.

relative arrangement of their constituent innous coal is such a compound which subsethe air and isconsumed. Then also the more 200 F. below red heat, the latter temperature being the lowest, at which any distillation of coal can be conducted) a smaller proportion of such hydrocarbons is thus decomposed, the ultimate result is, in quantity and quality of the product, not increased, because by a process of distillation, at such low temperatures, again a correspondingly larger proportion of the hydrocarbons is then not separated or removed from the carbon and the mineral constituents forming the fibrous and )orous structure of the coal. This explains w hy'the quantitative yield of such hydrocarbon products is not appreciably larger in distilling at low temperatures than in distilling at high temperatures, and also why such dlstilling processes were found not suitable for commercially recovering such hydrocarbons as are contained in cannel coal and other similarly constituted bituminous compounds. To obtain all hydrocarbon in redients of cannel coal, .and

'other similarly constituted materials, and

to recover them in a chemically unchanged condition, I sub]ect such bitumlnous raw material, in an atmosphere of neutral (deoxidized). gases, to a temperature only suflicient to render these hydrocarbons fluid, and then to suctionby a strong, mechanically produced current of these neutral gases, whereby the hydrocarbons, having been rendered sufficiently fluid by the heating, are separated and removed from the solid constituents of the material treated. The suction, created by the current, materially reduces the pressure in the chamber, where t he bituminous raw material is thus treated, thus creating a condition favorable to expansion and assists also materially in extracting the hydrocarbons of higher degree of consistency from among the fibers and pores of its carbon structure. The neutral gases, enveloping the hydrocarbons thus extracted, constantly, during this' transitory period, while they are in this heated and fluid state, prevent ther oxidation, and neutralize their tendency t split and form other chemical compound Finally, the hydrocarbons are separat from the protecting neutral gases by corldensation. This is effected by cooling the current of neutral gases, conveying the hydrocarbons in their fluid state, though a large proportion of the specifically heavier hfydrocarbons is quite rapidly precipitated rom the gaseous vehicle as soon as the velocity of the current is diminished, The chemical composition of hydrocarbon constituents of cannel coal and of similar bituminous materials thus recovered, is not changed, or in any respect materially modified. They are recovered in their crude state, and to render them available for further industrial uses, they must be separated from each other and refined. The processes for separating and-for refining art of the invention set forth erein, and therefore, are not them are no and claimed described.

An apparatus suitable for carryin on this eduction process is shown in the rawing, illustrating a vertical transverse section thereof, and consists, essentially, of an eduction chamber B, designed to be hermetically closed after the charge of the cannel coal or 'of a similar bituminous material was placed therein; an exhauster F, connected by a conduit 14' with the bottom part E of the eduction chamber; chambers 1 for producingor heating the neutral (deoxidized) gases; flues L for conveying these neutral gases into the eduction chamber, and devices (valves 26) for governing their admission.

The apparatus, designed by me for experimental practice of the process, herein set forth, and to demonstrate its industrial and commercial-utility, is shown and more fully described in the aforementioned Letters Patent No. 821,323, grantedto my assignees, the American Chemical Eduction 00., May 22, 1906. The apparatus was designed particularl with the object in view to em loy deoxi ized combustion gases, produce by the fires in -cham'bers'l, as such neutral ases, and comprises, in addition'to the above-re cited essentials,.the fuel magazines H, one set above each of the chambers 1 and rovided with flanged lids 20, entering into t e circular water trou hs 19; and a crate C, provided with brac rets 36, fixed to its sides, for supporting trays 37 whereon the raw material is 'disposed in comparativelythin la ers. The crate C is dimensioned to fit and til the interior of'the eduction chamber-B, its expansion by heat being considered; the trays '37 are made shorter than the longitudinal "width of the crate, and are set therein so that their ends arealternatel flush with one end of the crate. The con uits 22 for admission of the deoxidized combustion ases .enter the eduction chamber at the top, a ove the first tray,- and the conduit, connecting the eduction chamber with the exhauster, starts from bottom art E, below the last tray; consequently, tet-rays act as baffling plates, divertin zig-zag course through the charge, before the gases are drawn out by the exhauster. By this arrangement of the trays in the' eduction chamber, a more rapid and also quantitatively'somewhat more exhaustive progress 120 "is made in the eduction process.

In-the apparatus constructed as shown in the drawin s, the fires are started in chambers 1, the ues, leading to the chimney, be-

in then'open, and' the apertures 22 in the 125 si e walls of the eduction chamber shut. When the fires are suflici'ently developed, the chimney flues are shut, and only such a volume of air is admitted through the grates as the flow of the gases in a brought to a temperature of about 750 F.

erases fuel, safely deprived of all oxygen and} Then the valves 26one in each of the valve chambers M on to of the eduction chamber B-are opened and the exhauster F started, whereby the deoxidized combustion gases are drawn in a forced current'through the charge of the material, exposed to their action in the eduction chamber, and already sufiicientl heated, to render the hydrocarbons fluid to the extent required for drawing them out big suction and carry them into a condenser. uring this transitive period, while the hydrocarbons are in a heated condition, they are enveloped by the deoxidized gases, which thus protect them from oxidation, and also neutralize their 'tendency to split and recombine. This protection continues until the hydrocarbons are separated from the gases by coolin and condensation.

The crude roduct 0 this process is an aggregation o hydrocarbons of the paraffin series. They are of the same chemical composition as they were contained in the bituminous substance, treated in the process; and range in consistency from solid paraflins to light oils of the same series. Besides these hydrocarbons the crude product contains some carbolic acid and bodies of the chinolin and acridin class, The total of these crude products averages Well up to ninety per cent. of the difference between the weight of the bituminous material when charged into the apparatus and the weight of its dry residue when the eduction process is completed. The products of the cduction process are readily separated from each other and may be refined by any of the processes usually employed in this art. The aggregate of the purified and separated products should be about eighty per cent. of the crude product.

I claim as my invention:

1. The process for recovering, from cannel coal and similarly constituted bituminous compounds, their hydrocarbon ingredients of the paraflin series in chemically unchanged condition; the rocess consisting of the following steps :-(1 subjecting the material, from which the hydrocarbon ingredients are to be recovered, in an atmosphere of neutral (deoxidizcd) gases, to a temperait; drawing out, while continuing the current of neutral gases the fluid ingredients of the material with the neutral gases; and (4) separating them from the neutral gases, all substantially as herein set forth. I

2. The process for recovering from cannel coal and similarly constituted bituminous ccmpounds, their hydrocarbon ingredients 0 changed condition; the process consisting of the following steps l) enveloping the material, from which: the hydrocarbon ingredients are to be recovered, by neutral (deoxidized) gases; (2) then subjectin the material to a current of neutral eoxidized) gases and heating it to a temperature sufficient only to render its hydrocarbon ingredients fluid (3) drawing out, while continuing the current of neutral gases, the fluid ingredients of the material with the neutral gases; and (4) separating them from the neutral gases, all substantially as herein-set forth.

3. The process for recovering from cannel coal and similarly constituted bituminous compounds, their hydrocarbon ingredients of the parafiin series in chemically unchanged condition; the process consisting of the following steps 1) subjecting the material, from which the hydrocarbon ingredicuts are to be recovered, to a current of neutral (deoxidized) gases heated to not more than 750 F., whereby its hydrocarbon ingredients are rendered fluid; (2) drawing out, While continuing the current of neutral gases, the fluid ingredients of the material with the'neutral gases; and (3) condensing the recovered mixture, whereby the hydrocarbons are separated from the neutral. gases, all substantially as herein set forth.

In testimony that I claim the invention above set forth I have affixed my signature, in presence of two witnesses.

HENRY WURTZ.

Witnesses:

' ADAM WIENER, ARTHUR Lawn.

the paraflin series in chemically un- 

